The use of small scale renewable sorbent material for automated solid phase extraction of multi-residue pharmaceuticals in environmental samples exploiting the sequential injection analysis-bead injection with direct coupling to liquid chromatography-electrospray ionization tandem mass spectrometry (SIA-BI-μSPE-LC-ESI-MS/MS) is presented to determine beta-blockers, namely atenolol, sotalol, pindolol, acebutolol, timolol, metoprolol, labetalol, carazolol, propranolol and betaxolol. These compounds yielded the same product ions, therefore were affected in terms of quantification when flow injection analysis-mass spectrometry (FIA-MS) was used. Thus, analytes and matrix present in the sample travel together into the ionization source which can seriously affect the ionization efficiency and analyte signals due to monitoring over a short time period. Graphical abstract A two-dimensional analysis involving a time dimension (retention time) and an m/z dimension (fragmentation ion) is promising for the various sample types. Using the developed method, absolute recoveries percentages of 10 mL of sample loading volume were >91% for all β-blockers with enrichment factor of 62-74, limits of detection of 0.005-0.07 μg L(-1), limits of quantification of 0.01-0.23 μg L(-1), enrichment factor of 62-72 and repeatability within range 7-12%. This developed method is suggested to be used as quantitative screening technique for drugs of abuse or persistent contamination using different kinds of sorbent materials and complex matrix such as biological fluid sample as well.

Department of Analytical Chemistry Faculty of Pharmacy Charles University Prague Heyrovského 1203 500 05 Hradec Králové Czech Republic

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